EP0233394B1 - Adsorbeur pour purifier des gaz contenant du HC1 - Google Patents

Adsorbeur pour purifier des gaz contenant du HC1 Download PDF

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Publication number
EP0233394B1
EP0233394B1 EP86302984A EP86302984A EP0233394B1 EP 0233394 B1 EP0233394 B1 EP 0233394B1 EP 86302984 A EP86302984 A EP 86302984A EP 86302984 A EP86302984 A EP 86302984A EP 0233394 B1 EP0233394 B1 EP 0233394B1
Authority
EP
European Patent Office
Prior art keywords
scavenger
hci
alumina
gas
promoter
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP86302984A
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German (de)
English (en)
Other versions
EP0233394A2 (fr
EP0233394A3 (en
Inventor
Michael John Pearson
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Laroche Chemicals Inc
Original Assignee
Laroche Chemicals Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Laroche Chemicals Inc filed Critical Laroche Chemicals Inc
Publication of EP0233394A2 publication Critical patent/EP0233394A2/fr
Publication of EP0233394A3 publication Critical patent/EP0233394A3/en
Application granted granted Critical
Publication of EP0233394B1 publication Critical patent/EP0233394B1/fr
Expired legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/68—Halogens or halogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite

Definitions

  • HCI gaseous HCI
  • a chlorine-promoted catalyst generally platinum
  • HCI hydrogen-promoted catalyst
  • This reforming operation also generates hydrogen which is usually recycled to the reforming reactor. Even if this recycled portion only contains the HCI impurity in small amounts, it can seriously interfere with the operation and can also cause corrosion upon contact with the moisture content of the gas.
  • active alumina was found to be suitable as a scavenger for the removal of small quantities of HCI from gaseous streams.
  • compositions comprising an alumina component and a salt or mixture of salts of alkali or alkaline earth metals as scavengers is known from US-A-4 323 544, but this use is disclosed in relation to the removal of nitrogen oxides and sulphur oxides from waste gases.
  • sodium, potassium and the other alkali metals are disadvantageous as promoters for alumina, in comparison with calcium, magnesium and the other alkaline earth metals, because the alkali metal compounds associated with the alumina react with water vapour, which is almost invariably present in waste gases, causing these scavengers to disintegrate. This difficulty does not arise with the promoted scavengers of the present invention.
  • the alkaline earth metal salt promoted aluminous materials of the present invention exhibit a significantly higher HCI scavenging property than the prior art scavengers and simultaneously exhibit an increased stability in the presence of moisture under the scavenging conditions generally employed.
  • a process for purifying industrial gases containing HCI as a contaminant which comprises contacting gas, containing up to about 1% by volume of HCI, with an alumina-containing scavenger, is characterised in that the scavenger contains 0.5% to 45% by weight of alkaline earth metal, as a promoter, it is subjected to thermal activation prior to contact with the gas and, in the thermally-activated state, the scavenger exhibits a minimum surface area of about 50 m 2 /g and a minimum pore volume of about 0.3 cm 3 /g and in that contact between the HCI-contaminated gas and the thermally-activated scavenger is maintained until the HCI content of the gas reaches a predetermined threshold level, after which the scavenger containing the HCI impurity removed from the gas is recovered.
  • the alkaline earth metal salt promoted alumina-containing scavenger contains 0.5 to 45% by weight of alkaline earth metal salt calculated as the metal.
  • the alkaline earth metal present is calcium or magnesium.
  • the scavenger can remove up to about 20% by weight of CI from gas streams contaminated with up to about 1 % by volume HCI.
  • the alkaline earth metals can be added as their salts to the bauxite or alumina in a convention manner, such as by impregnation.
  • Shaped promoted scavenger material can also be made by admixing the desired quantity of promoter with the bauxite or alumina, followed by shaping, for example, nod- ulization or extrusion, and subsequent thermal activation.
  • alumina-containing material refers to both bauxite and to alumina (Al Z O 3.x H 2 O) derived from bauxite or any other alumina-bearing source, such as beneficiated clays.
  • alkaline earth metal or "promoter” as used herein refer to the metals of Group IIA of the Periodic Classification of the Elements, the preferred alkaline earth metals being calcium and magnesium.
  • Suitable alumina-containing materials which can be advantageously employed for making the promoted scavenger include both bauxite and Al 2 0 3 .xH 2 0, provided these materials meet certain criteria.
  • bauxite when bauxite is utilized, it should have a minimum alumina (AI 2 0a) content of about 40% by weight, calculated on the basis of its dry weight; i.e. after ignition at 1000 ° C for 1 hour.
  • the silica (Si0 2 ) content of the bauxite should not exceed 15% by weight on the dry basis.
  • Suitable bauxites include those mined in the Caribbean, South America, Australia and Western Africa.
  • alumina When alumina is utilized for preparation of the promoted scavenger, it can be derived from alumina trihydrate (Al ⁇ Os. 3H 2 0) manufactured by the well-known Bayer process or it can be a gel-type alumina made by the neutralization of a basic aluminum salt with an acid or an acidic aluminum salt with a base.
  • Typical aluminas, suitable for use as the base material for the promoted scavenger include without limitation alumina trihydrate, pseudoboehmite, alpha alumina monohydrate and other well-known thermally-activated aluminas exhibiting gamma, chi-rho-eta, delta or kappa structures.
  • the promoted scavenger after thermal activation, should exhibit a minimal surface area of 50 m 2 /gram, preferably having a surface area in excess of about 100 m 2 /g.
  • the promoted scavenger should also have a minimum pore volume, again after thermal activation, of about 0.3 cm 3 /g, preferably in the range from about 0.4 to about 0.6 cm3 / g.
  • alkaline earth metals suitable as promoters for the HCI scavenger are those in Group IIA of the Periodic Table and thus include calcium, strontium, magnesium and barium, calcium and magnesium being the most preferred metals.
  • incorporación of the promoter in the alumina-containing material can be accomplished in the conventional manner, for example by impregnation or by admixture of the promoter with the alumina-containing material followed by shaping. If impregnation is employed as the means for promoting the scavenging capabilities of the alumina-containing material, then the alkaline earth metal is generally employed in the form of a water-soluble compound or salt.
  • Suitable alkaline earth metal compounds and salts which lend themselves for impregnation from an aqueous solution include the hydroxides, nitrates, chlorides, acetates and the salts of other organic acids, those salts being preferred which can be readily decomposed to the corresponding oxides under relatively low temperature thermal activation without generating environmentally harmful offgases.
  • Aqueous alkaline earth metal salt solutions can be employed or, if desired, the alumina-containing material can be in granular form and, after impregnation, the material can be shaped.
  • the promoter can be admixed in dry form with the alumina-containing material followed by shaping into any desired form by the well-known shaping processes. Also, the promoter and the alumina-containing material can be condulized to form HCI scavenging nodules.
  • the quantity of promoter to be added to the alumina-containing material can range from about 0.5% to about 45% by weight, based on the alkaline earth metal content of the promoted scavenger. Particularly good HCI scavenging results can be achieved when the promoter is present in the composite in an amount from about 1% to about 20% by weight, calculated as the metal and based on the weight of the composite.
  • a thermal activation step is generally utilized for the preparation of the promoted scavenger.
  • the thermal treatment is required particularly when the alumina-containing material utilized for the promoted scavenger is a bauxite in the unactl- vated state or an alumina of high bound and unbound water content, such as Bayer hydrate (AI Z O s .3H z 0) or gel alumina.
  • the alumina-containing material used for making the scavenger composition is a previously activated alumina or bauxite
  • impregnation with an aqueous promoter solution or shaping in the presence of water makes it necessary to subject the promoted scavenger to a thermal treatment step.
  • the thermal treatment or activation step not only imparts increased activity to the scavenger, but also accomplishes the thermal decomposition of the alkaline earth metal salt to the corresponding oxides.
  • temperatures in the range from about 150 ° C to about 500 ° C are utilized, depending on the decomposition temperature of the alkaline earth metal salts employed and the nature of the alumina-containing material used for the scavenger.
  • the thermally treated or activated scavenger can be readily employed in the removal of HCI impurities from industrial offgases. Generally, removal is accomplished by providing an adsorber vessel charged with the scavenger and the HCI contaminated gases are conducted through the adsorber either in a down or in an upflow manner. The exit gas will be free of HCI which will be removed by the scavenger of the instant invention. It has been observed that the best scavenging activity can be achieved by treating gas streams containing up to about 1% by volume HCI impurity. Larger quantities of HCI impurity in the gas streams may cause premature saturation of the promoted scavenger with the possibility of having an undesired early break-through and consequent corrosion and environmental problems.
  • the promoted scavenger of the invention is effective in removing HCI from gas streams containing the same as impurity in amounts less than 1.0% by volume to levels of less than 1 ppm by weight thus providing an offgas of significantly reduced HCI content. Further, it has also been found that if the HCI contamination of the gas is in the range from about 2 to about 4 ppm, the scavenger is still capable of reducing this very small HCI concentration to levels below the 1 ppm limit.
  • Purification of HCI contaminated gas streams with the promoted scavenger is generally continued until the gas exiting from the purifying column is observed to have an HCI content above the desired level.
  • the gas to be purified is conducted into a column filled with fresh promoted scavenger and the scavenger saturated with HCI is either discarded or employed for other purposes.
  • the HCI contaminated scavenger can be subjected to a purification process involving dissolution of the alumina content and the recovery of the same.
  • transitional alumina nodules having a chi-rho-eta crystal structure, were used as the alumina-containing material for the promoted scavenger.
  • the transitional alumina nodules were prepared from alumina trihydrate by the method described in U.S. patent 3,222,129. Batches of these nodules, exhibiting a surface area of 360 m 2 /g and a pore volume of 0.48 cm 3 /g, were then combined with Ca, Mg and Ba promoters by the impregnation method using the water-soluble acetate salts of these alkaline earth metals. Impregnation was followed by drying at 110°C and subsequent thermal treatment at 400 ° C for 2 hours.
  • Each impregnated batch of promoted scavengers was then tested for HCI adsorption capacity by charging separate adsorption columns with each type of promoted scavenger an using an HCI-contaminated reforming gas for purification purposes.
  • the gas such as used in the catalytic reforming of hydrocarbons, contained 0.1% volume HCI and 1000 ppmv water vapor. Purification of the gas was carried out at room temperature until the break-through point which was established as 1 ppm HCI in the purified gas. The chloride content of the exhausted scavenger was then analytically determined. For comparison purposes a column filled with unimpregnated transitional alumina nodules was also used for HCI removal from the same type of gas as used for testing the promoted scavengers. The results were tabulated and are shown in Table I.
  • bauxite was utilized as the alumina-containing portion of the promoted scavenger.
  • the bauxite utilized has a composition shown in Table II.
  • the bauxite was dried at 110°C, then ground to a suitable particle size.
  • the ground bauxite was then admixed with an aqueous suspension of Ca(OH) 2 and the mixture was formed into adobe shapes by pressing.
  • the adobes were dried at about 110 ° C for 1 hour, then subjected to thermal activation for about 1 hour at 400 ° C.
  • the shaped and activated calcium-promoted bauxite scavenger was then charged into a column and HCI-contaminated gas was conducted through the column until break-through was observed by analyzing the gas exiting the column.
  • the HCI-contaminated gas had an HCI content of 0.2% and a moisture content of 2000 ppmv.
  • the exit gas had a less than 1 ppm HCI content until the break-through point was reached. Purification of the gas was accomplished at ambient temperature.
  • a control test was also conducted with the same bauxite, however no promoter was used to increase its HCI scavenging ability. The results of the scavenging tests are shown in Table III.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Biomedical Technology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Treating Waste Gases (AREA)
  • Gas Separation By Absorption (AREA)
  • Industrial Gases (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Catalysts (AREA)

Claims (6)

1. Procédé d'épuration de gaz industriels contenant du HCI comme impureté, qui consiste à mettre en contact un gaz contenant jusqu'à environ 1 % en volume de HCI avec un accepteur contenant de l'alumine, caractérisé en ce que l'accepteur contient 0,5 à 45 % en poids de métal alcalino-terreux comme activateur, est exposé à une activation thermique avant sa mise en contact avec le gaz et présente, à l'état activé thermiquement, une surface spécifique minimale d'environ 50 m2/g et un volume minimal des pores d'environ 0,3 cm3/g, et en ce que le contact entre le gaz contaminé par du HCI et l'accepteur activé thermiquement est maintenu jusqu'à ce que la teneur en HCI du gaz atteigne un seuil prédéterminé, après quoi l'accepteur contenant le HCI comme impureté éliminé du gaz est récupéré.
2. Procédé suivant la revendication 1, dans lequel l'accepteur comprend de la bauxite, de l'alumine tri- hydratée, de la pseudoboehmite, de l'alpha-alumine monohydratée ou leurs mélanges.
3. Procédé suivant la revendication 1 ou 2, dans lequel l'activateur contenant un métal alcalino-terreux est présent en une quantité comprise dans la plage de 1 à 20 % par rapport au poids de l'accepteur.
4. Procédé suivant la revendication 1, 2 ou 3, dans lequel le métal alcalino-terreux est le calcium ou le magnésium.
5. Procédé suivant l'une quelconque des revendications précédentes, dans lequel l'accepteur est de la bauxite activée thermiquement ou une alumine de transition de structure chi-rho-êta, et l'activateur est le calcium.
6. Procédé suivant la revendication 5, dans lequel l'activateur renferme du magnésium.
EP86302984A 1985-10-09 1986-04-21 Adsorbeur pour purifier des gaz contenant du HC1 Expired EP0233394B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/785,706 US4639259A (en) 1985-10-09 1985-10-09 Promoted scavenger for purifying HCl-contaminated gases
US785706 1997-01-17

Publications (3)

Publication Number Publication Date
EP0233394A2 EP0233394A2 (fr) 1987-08-26
EP0233394A3 EP0233394A3 (en) 1988-03-30
EP0233394B1 true EP0233394B1 (fr) 1990-09-05

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP86302984A Expired EP0233394B1 (fr) 1985-10-09 1986-04-21 Adsorbeur pour purifier des gaz contenant du HC1

Country Status (6)

Country Link
US (1) US4639259A (fr)
EP (1) EP0233394B1 (fr)
JP (1) JPH0618639B2 (fr)
AU (1) AU576165B2 (fr)
CA (1) CA1239771A (fr)
DE (1) DE3673985D1 (fr)

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Also Published As

Publication number Publication date
CA1239771A (fr) 1988-08-02
DE3673985D1 (de) 1990-10-11
EP0233394A2 (fr) 1987-08-26
US4639259A (en) 1987-01-27
JPS6287244A (ja) 1987-04-21
EP0233394A3 (en) 1988-03-30
AU6356486A (en) 1987-04-16
JPH0618639B2 (ja) 1994-03-16
AU576165B2 (en) 1988-08-11

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